CN113877489B - Air inlet device for organic silicon fluidized bed and fluidization method - Google Patents
Air inlet device for organic silicon fluidized bed and fluidization method Download PDFInfo
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- CN113877489B CN113877489B CN202111387545.9A CN202111387545A CN113877489B CN 113877489 B CN113877489 B CN 113877489B CN 202111387545 A CN202111387545 A CN 202111387545A CN 113877489 B CN113877489 B CN 113877489B
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- air inlet
- fluidized bed
- side wall
- gas
- pipes
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000005243 fluidization Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 title description 8
- 239000010703 silicon Substances 0.000 title description 8
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 17
- 229920001296 polysiloxane Polymers 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 19
- 239000002245 particle Substances 0.000 abstract description 8
- 239000008247 solid mixture Substances 0.000 abstract description 7
- 230000005484 gravity Effects 0.000 abstract description 4
- 238000007664 blowing Methods 0.000 abstract description 3
- 229940050176 methyl chloride Drugs 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000005465 channeling Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1818—Feeding of the fluidising gas
- B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
- B01J8/38—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it
- B01J8/384—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it being subject to a circulatory movement only
- B01J8/386—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it being subject to a circulatory movement only internally, i.e. the particles rotate within the vessel
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention provides an air inlet device and a fluidization method for an organosilicon fluidized bed. Before the raw material gas enters the fluidized bed reactor, most of chloromethane gas in the raw material gas enters the fluidized bed reactor as spouted gas through the middle air inlet pipe, and the rest of chloromethane gas enters the fluidized bed reactor as fluidized gas through the side wall air inlet pipes. Wherein the spouted gas causes the gas-solid mixture in the fluidized bed to generate spouted fluidization, and simultaneously the gas-solid mixture is blown to a higher position in the fluidized bed for reaction. The fluidization gas allows the particles in the fluidized bed to fluidize normally while blowing the raw material falling back by gravity to the center again. According to the invention, silicon powder cannot stay and accumulate in the fluidized bed, so that the problem that the silicon powder forms a dead zone on the gas distributor in the prior art is solved, and the normal reaction of the fluidized bed is ensured.
Description
Technical Field
The invention relates to the technical field of organosilicon synthesis devices, in particular to an air inlet device for an organosilicon fluidized bed and a fluidization method.
Background
The reactor for synthesizing the organosilicon monomers generally adopts a fluidized bed reactor, but the fluidized bed reactor adopted at home at present has unreasonable structure. The fluidized bed body is mostly a cylinder or a combination of a cylinder and a cone, and a gas distributor is arranged at the bottom of the fluidized bed and is generally a flat plate open-pore type or cone sieve plate type gas distributor. During use, if the velocity of the fluidizing gas does not reach the initial fluidization velocity of those larger particles, or if there are particles that are not fluidized, they can deposit on the distribution plate creating dead zones. In the high-temperature organic silicon monomer synthesis reaction, raw material gas chloromethane and byproducts generated by the reaction are heated and decomposed at high temperature to carbonize, so that silicon powder particles and carbon are combined into blocks, the vent holes on a distribution plate are blocked by the silicon powder blocks, channeling is caused when the silicon powder blocks are serious, the fluidization quality is rapidly deteriorated, the selectivity of the product is also rapidly reduced, a larger dead zone is generated, and the agglomeration phenomenon of the silicon powder particles is also more serious.
Disclosure of Invention
In view of the above, the invention provides an air inlet device for a silicone fluidized bed and the silicone fluidized bed, which can overcome the problems that silicon powder particles form dead areas on a distribution plate, block ventilation holes and seriously influence the selectivity of products.
In order to solve the problems, the invention provides the following technical scheme.
In a first aspect, the invention provides an air inlet device for an organosilicon fluidized bed, wherein the lower end of the organosilicon fluidized bed is a lower cone, and the air inlet device comprises a middle air inlet pipe and a plurality of side wall air inlet pipes;
wherein the middle air inlet pipe is arranged at the bottom of the lower cone; the side wall air inlet pipes are arranged on the side wall of the lower cone, and are uniformly distributed along the circumferential direction of the lower cone.
Further, the middle air inlet pipe is used for feeding silicon powder and chloromethane gas into the fluidized bed, and the side wall air inlet pipes are used for feeding chloromethane gas into the fluidized bed.
Further, the air inflow of the methyl chloride gas of the middle air inlet pipe accounts for 65-75 wt.% of the total amount of the raw material gas, and the total air inflow of the methyl chloride gas of the side wall air inlet pipe accounts for 25-wt wt.% of the total amount of the raw material gas.
Further, the number of the side wall air inlet pipes is 4-100.
Further, the angle of the cone angle theta of the lower cone in the organosilicon fluidized bed is 30-80 degrees.
Further, a part of the side wall air inlet pipe vertically extends into the organosilicon fluidized bed, and the extending height is not more than the plane formed by the upper edge of the lower cone.
Further, a valve is arranged on the middle air inlet pipe, and the air inflow of the middle air inlet pipe can be controlled through the valve.
Further, the air inlet device further comprises a plurality of connecting pipes, the connecting pipes are connected with the side wall air inlet pipes, the number of the connecting pipes is the same as that of the side wall air inlet pipes, the connecting pipes are provided with valves, and the air inlet amount of the side wall air inlet pipes can be controlled through the valves.
Further, the ratio of the pipe diameter of the middle air inlet pipe to the pipe diameter of the side wall air inlet pipe is (3-20): 1.
in a second aspect, the present invention provides a silicone fluidised bed comprising an air inlet means as described above.
The technical scheme of the invention has the following beneficial effects:
the invention provides an air inlet device for an organic silicon fluidized bed and the organic silicon fluidized bed, wherein the lower end of the organic silicon fluidized bed is a lower cone, and the air inlet device comprises a middle air inlet pipe and a plurality of side wall air inlet pipes; wherein the middle air inlet pipe is arranged at the bottom of the lower cone; the side wall air inlet pipes are arranged on the side wall of the lower cone, and are uniformly distributed along the circumferential direction of the lower cone. Compared with the existing fluidized bed air inlet device, the air inlet device provided by the invention omits the air distributor, 65-75 wt.% of chloromethane gas in the raw material gas is taken as spraying air to enter from the middle air inlet pipe before the raw material gas enters the fluidized bed reactor, and the rest 25-wt-35-wt% of chloromethane gas is taken as fluidization air to enter from the side wall air inlet pipes. Wherein the spouted gas causes spouted fluidization of the gas-solid mixture in the fluidized bed, and simultaneously, the gas-solid mixture is easily blown to a higher position in the fluidized bed for reaction. The fluidization gas allows the particles in the fluidized bed to fluidize normally while blowing the raw material falling back by gravity to the center again. In the invention, the silicon powder circulates under the action of the spouted gas and the fluidization gas, and the bottom of the fluidized bed is a cone, so that the silicon powder cannot stay and accumulate in the fluidized bed, the problem that the silicon powder forms dead zones on a gas distributor in the prior art is solved, and the normal reaction of the fluidized bed is ensured.
Drawings
FIG. 1 is a schematic structural view of a silicone fluidized bed;
fig. 2 is a top view of the lower cone in the silicone fluidized bed.
Reference numerals:
the device comprises a lower cone 1, a middle air inlet pipe 2, a side wall air inlet pipe 3 and a connecting pipe 4.
Description of the embodiments
For a further understanding of the present invention, preferred embodiments of the invention are described below in conjunction with the examples, but it is to be understood that these descriptions are merely intended to illustrate further the features and advantages of the invention and are not limiting of the invention.
The fluidized bed air inlet device in the present invention will be further described with reference to fig. 1 and 2.
In a first aspect, the invention provides an air inlet device of a fluidized bed, as shown in fig. 1, wherein the lower end of the fluidized bed is a lower cone 1, and the air inlet device comprises a middle air inlet pipe 2 and a plurality of side wall air inlet pipes 3; wherein the middle air inlet pipe 2 is arranged at the bottom of the lower cone 1; the side wall air inlet pipes 3 are arranged on the side wall of the lower cone 1, and the side wall air inlet pipes 3 are uniformly distributed along the circumferential direction of the lower cone 1.
According to some embodiments of the invention, the middle gas inlet pipe 2 is used for feeding silicon powder and chloromethane gas into the fluidized bed, and the plurality of side wall gas inlet pipes 3 are used for feeding chloromethane gas into the fluidized bed.
According to some embodiments of the present invention, the air intake amount of the methyl chloride gas in the middle air intake pipe 2 is 65wt.% to 75wt.% of the total amount of the raw material gas, and the total air intake amount of the methyl chloride gas in the side wall air intake pipe 3 is 25 wt.% to 35wt.% of the total amount of the raw material gas.
In particular, the invention provides an air inlet device of the fluidized bed, which has a much simplified structure compared with the existing fluidized bed and omits a gas distributor at the lower part of the existing fluidized bed. The invention takes a fluidized bed with a lower cone 1 at the lower end as a basic structure for improvement, a middle air inlet pipe 2 is arranged at the bottom of the lower cone 1 of the fluidized bed, in the reaction process, the middle air inlet pipe 2 is used for feeding silicon powder and chloromethane gas, meanwhile, the middle air inlet pipe 2 is a spouted air pipe, the air quantity of the middle air inlet pipe 2 is larger, spouted air in the middle air inlet pipe 2 ensures that reaction raw materials (silicon powder, chloromethane gas and gas-solid mixture) in the fluidized bed are spouted and fluidized on one hand, and on the other hand, the reaction raw materials can be blown to a higher position in the fluidized bed, and the specific height is the level with the top of a heat exchanger in the fluidized bed. The fluidized bed air inlet device of the invention utilizes a jet of jet air jetted by the middle air inlet pipe 2 to jet the reaction raw materials into the fluidized bed from the center, and the existing fluidized bed needs to utilize the blown air to horizontally push the reaction raw materials filled in the fluidized bed to a certain height, so that the fluidized bed air inlet device provided by the invention is easier to blow the reaction raw materials to the same reaction height. Meanwhile, as shown in fig. 2, the fluidized bed air inlet device of the invention further comprises a plurality of side wall air inlet pipes 3 arranged on the side wall of the lower cone 1 of the fluidized bed, wherein the side wall air inlet pipes 3 are uniformly distributed along the circumferential direction of the lower cone 1, and the side wall air inlet pipes 3 are used for feeding chloromethane gas. In the reaction process, the air inflow of the side wall air inlet pipe 3 is smaller than that of the middle air inlet pipe 2, and the air inflow of the side wall air inlet pipe 3 serves as fluidization air to play a role in fluidization. The raw materials conveyed into the fluidized bed by the middle air inlet pipe 2 fall back due to the action of gravity, and the blown air in the side wall air inlet pipe 3 can blow the fallen raw materials to the center again for continuous circulation.
In summary, compared with the existing fluidized bed air inlet device, the air inlet device provided by the invention omits the air distributor, 65-75 wt.% of chloromethane in the raw material gas is taken as spouted air from the middle air inlet pipe 2 before the raw material gas enters the fluidized bed reactor, and the rest 25-wt-35-wt wt.% of chloromethane is taken as fluidized air from the side wall air inlet pipes 3. Wherein the spouted gas causes spouted fluidization of the gas-solid mixture in the fluidized bed, and simultaneously, the gas-solid mixture is easily blown to a higher position in the fluidized bed for reaction. The fluidization gas allows the particles in the fluidized bed to fluidize normally while blowing the raw material falling back by gravity to the center again. In the invention, the silicon powder circulates under the action of the spouted gas and the fluidization gas, and the bottom of the fluidized bed is a cone, so that the silicon powder cannot stay and accumulate in the fluidized bed, the problem that the silicon powder forms dead zones on a gas distributor in the prior art is solved, and the normal reaction of the fluidized bed is ensured.
According to some embodiments of the present invention, the number of the sidewall air inlet pipes 3 is 4-100. In the present invention, the number of the side wall air inlet pipes 3 is set according to the actual situation, and preferably the number of the side wall air inlet pipes 3 is 8. The sidewall inlet pipe 3 may be uniformly distributed on the sidewall of the lower cone 1 along the circumferential direction, and divided into inner and outer layers, as shown in fig. 2. At the same time, the side walls of the lower cone 1 can be uniformly distributed along the circumferential direction, and only one layer is distributed. In practical applications, the specific distribution manner of the sidewall air inlet pipes 3 may be selected according to the total number of the sidewall air inlet pipes 3.
According to some embodiments of the invention, the angle of taper θ of the lower cone 1 in the fluidized bed is 30 ° to 80 °. In order to prevent silicon powder from staying or even accumulating on the side wall of the lower cone 1 during the reaction, the taper angle θ of the lower cone 1 in the present invention needs to be set at an acute angle. Specifically, the angle of the taper angle θ of the lower cone 1 in the fluidized bed is 30 ° to 80 °, and the angle of the taper angle θ of the lower cone 1 is preferably 45 ° as proved by experiments.
According to some embodiments of the invention, the portion of the side wall inlet pipe 3 extends vertically into the silicone fluidized bed by a height not exceeding the plane formed by the upper edge of the lower cone 1. In the invention, a part of the side wall air inlet pipe 3 vertically extends into the organosilicon fluidized bed, and the height of the side wall air inlet pipe 3 is not more than the plane based on the plane formed by the upper edge of the lower cone 1.
According to some embodiments of the invention, a valve is arranged on the middle air inlet pipe 2, and the air inflow of the middle air inlet pipe 2 can be controlled through the valve.
According to some embodiments of the present invention, the air intake device further includes a plurality of connection pipes 4, the connection pipes 4 are connected to the sidewall air intake pipes 3, the number of the connection pipes 4 is the same as the number of the sidewall air intake pipes 3, each connection pipe 4 may be connected to a corresponding sidewall air intake pipe 3, a valve is disposed on the connection pipe 4, and an air intake amount of the sidewall air intake pipe 3 may be controlled by the valve. The axis of the sidewall inlet pipe 3 and the axis of the middle inlet pipe 2 may be parallel to each other, and the axis of the middle inlet pipe 2 may be collinear with the axis of the lower cone 1.
In the actual reaction process, the amount of the reactant in the fluidized bed is changed, so that the air inflow in the middle air inlet pipe 2 needs to be regulated, the blown height of the reaction raw materials and the spouted fluidization effect are ensured, and the air inflow in the middle air inlet pipe 2 is regulated by adding a valve on the middle air inlet pipe 2. At the same time, the amount of intake air in the side wall intake pipe 3 also needs to be adjusted to accommodate the amount of reactant in the fluidized bed and ensure fluidization. Therefore, the air intake device in the present invention includes a plurality of connection pipes 4 connected to the side wall air intake pipe 3, and by providing valves on the connection pipes 4, the intake air amount of the side wall air intake pipe 3 can be controlled by the valves.
According to some embodiments of the present invention, the ratio of the pipe diameter of the middle air inlet pipe 2 to the pipe diameter of the side air inlet pipe 3 is (3-20): 1. in the invention, the middle air inlet pipe 2 is used as a spouted air pipe, the air quantity is larger, the side wall air inlet pipe 3 is used as a fluidized air pipe, the air quantity is smaller, and the ratio of the pipe diameter of the middle air inlet pipe 2 to the pipe diameter of the side wall air inlet pipe 3 is (3-20): 1, in practical application, the total number of the sidewall air inlet pipes 3 is also considered, and the pipe diameter of the sidewall air inlet pipes is adjusted.
In a second aspect, the present invention provides a silicone fluid bed comprising an air inlet arrangement as described above. The organosilicon fluidized bed may include a bed body and an air inlet device, the upper edge of the lower cone 1 may be connected with the edge of the opening of the lower end of the bed body, the axis of the bed body may be collinear with the axis of the lower cone 1, the sidewall air inlet pipe 3 may be disposed adjacent to the inner sidewall of the bed body, and the sidewall air inlet pipe 3 may be disposed spaced apart from the inner sidewall of the bed body in the radial direction of the bed body. Alternatively, the spacing distance between the side wall air inlet pipe 3 and the inner side wall of the bed body can be 1/8 to 3/5 of the radius of the bed body. Specifically, the structure of the organic silicon fluidized bed is shown in the attached figure 1, the organic silicon fluidized bed provided by the invention solves the problems that silicon powder is accumulated and blocked on a gas distributor to further form a dead zone in the prior art, realizes long-time and continuous reaction of the fluidized bed, and can ensure that the selectivity of a product is not reduced.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate a relative positional relationship, which changes accordingly when the absolute position of the object to be described changes.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (4)
1. The fluidization method for the organosilicon fluidized bed is characterized in that the lower end of the organosilicon fluidized bed is a lower cone, and the air inlet device comprises a middle air inlet pipe and a plurality of side wall air inlet pipes;
wherein the middle air inlet pipe is arranged at the bottom of the lower cone; the side wall air inlet pipes are arranged on the side wall of the lower cone, and are uniformly distributed along the circumferential direction of the lower cone; the number of the side wall air inlet pipes is 4-100; the air inlet device further comprises a plurality of connecting pipes, the connecting pipes are connected with the side wall air inlet pipes, the number of the connecting pipes is the same as that of the side wall air inlet pipes, valves are arranged on the connecting pipes, and the air inflow of the side wall air inlet pipes can be controlled through the valves;
the middle air inlet pipe is used for feeding silicon powder and chloromethane gas into the fluidized bed, and the side wall air inlet pipes are used for feeding chloromethane gas into the fluidized bed; the air inflow of the chloromethane gas of the middle air inlet pipe accounts for 65-75 wt.% of the total amount of the raw material gas, and the total sum of the air inflow of the chloromethane gas of the side wall air inlet pipes accounts for 25-wt wt.% to 35wt.% of the total amount of the raw material gas;
and a part of the side wall air inlet pipe vertically extends into the organosilicon fluidized bed, and the extending height is not more than the plane formed by the upper edge of the lower cone.
2. The fluidization method according to claim 1, wherein the angle of taper θ of the lower cone in the silicone fluidized bed is 30 ° to 80 °.
3. The fluidization method according to claim 1, wherein a valve is provided in the middle air intake pipe, and the amount of air taken in the middle air intake pipe can be controlled by the valve.
4. The fluidization method according to claim 1, wherein the ratio of the pipe diameter of the middle air intake pipe to the pipe diameter of the side wall air intake pipe is (3 to 20): 1.
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CN201140063Y (en) * | 2007-09-05 | 2008-10-29 | 青岛科技大学 | Bipyramid flow guiding type air inlet distributor of organosilicon monomer fluid bed reactor |
CN202638403U (en) * | 2012-07-02 | 2013-01-02 | 阎世城 | Gas distributing device of organic silicon fluidized bed |
DE102015224120A1 (en) * | 2015-12-02 | 2017-06-08 | Wacker Chemie Ag | Fluidized bed reactor and process for producing polycrystalline silicon granules |
CN209816042U (en) * | 2019-01-23 | 2019-12-20 | 江苏普格机械有限公司 | Reinforced bubbling internal circulation fluidized bed gasification furnace |
CN210058199U (en) * | 2019-04-04 | 2020-02-14 | 北京国化新材料技术中心(有限合伙) | Spout structure and fluidized bed |
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